液相色谱串联质谱法同时测定

DOI:10.3724/SP.J.1096.2010.00197A马强1白桦*1王超1张庆1周新1董辉2王宝麟1(,100123)2(,100088)A,,10.3MPa1202,SupelcleanEnviCarb,(14,V/V),WatersXBridgeC18,0.1%,,LC/MS/MSA0.5g/kg,0.5~10g/kg3,86.9%~92.5%,9.1%;87.8%~93.0%,8.8%,;;;;;;;A20090615;20090827(No.2007IK094)*Emai:[e-mail]1A,[1]A,,[2],[3,4],,[5],[6](OSPAR)[7]2003/53/EC0.1%[8]OekoTexStandard1000,[9]2008,A,A(PoHS)A,A(HPLC)[10,11](SFC)[12](MEC)[13](CE)[14](ELISA)[15](GC/MS)[16,17](LC/MS/MS)[18,19],[10][12,13,16,18][19][17],A,10minA,,22.1Alliance2695QuattromicroAPI(Waters);ASE3003820102(FENXIHUAXUE)ChineseJournalofAnalyticalChemistry2197~201(Dionex);N1000(Eyela),BC55(Yamato);TurboVap(Caliper);GX274ASPEC(Gilson);SupelcleanEnviCarb(6mL,500mg,Supelco);AcrodiscGHP(Pall);(99.999%)A4(99%,Sigma);4tert(98.5%,Dr.Ehrenstorfer);4(99%),(ChemService);4n(98%,AlfaAesar)(Fisher),MilliQ(0.22m);()2.2WatersXBridgeC18(150mm2.1mm,3.5m);:(A)0.1%(B):0~6min,30%~95%A;6~10min,95%A;10~12min,95%~30%A;12~15min,30%A0.2mL/min;25;5L;;3.10kV;0.5V;120;350;500L/h;50L/h;0.32kPa(Ar);(MRM),A11ATable1LC/MS/MSparametersfornonylpheno,loctylphenolandbisphenolAanalysisPhenolicxenoestrogensRetentiontime(min)Monitoringionpairs(m/z)Conevoltage(V)Collisionenergy(eV)PossibleidentityABisphenolA6.19227.0/132.9227.0/212.030302520[M-H-CH3]-[M-H-C6H6O]-4tert4tertOctylphenol8.15205.2/118.7205.2/132.735356525[M-H-C6H14]-[M-H-C5H12]-44Nonylphenol8.55219.2/132.7219.2/146.933333025[M-H-C6H14]-[M-H-C5H12]-44Octylphenol8.66205.2/105.7205.2/118.633332040[M-H-C7H16]-[M-H-C6H14]-4n4nNonylphenol9.05219.2/105.7219.2/118.635352042[M-H-C8H18]-[M-H-C7H16]-2.3,2.0g,34mL,,10.3MPa120,2,,,2mL,10mLV()V()=1410mL,10mLSupelcleanEnviCarb,2mLV()V()=14,1mL,020m,LC/MS/MS33.1A,,(30min)(30min)(12h)(2.3),,,((11,V/V)(37,V/V))(60,80,100,120140)(1,23),,C18(SupelcleanLCC18,SepPakC18)(OasisHLB)19838(SupelcleanEnviCarb)/(SepPakCarbon/NH2),SupelcleanEnviCarb10mL(14,V/V)10mL,10mL(2mL),(14,V/V),,,2mL3.2(XBridgeC18,SunFireC18,ZORBAXExtendC18,XBridgeC8,XBridgePhenyl)(ZORBAXNH2,SpherisorbS3W),AXBridgeC18(150mm2.1mm,3.5m)XBridge,,A,0.1%5mmol/L5mmol/L,0.1%A,H+(),,0.05%~0.5%,0.1%A/(Kow)3.32~5.92,,,10min1AMRMFig.1Multiplereactionmonitoring(MRM)chromatogramofnonylpheno,loctylphenolandbisphenolA1.A(BisphenolA);2.4tert(4tertOctylphenol);3.4(4Nonylphenol);4.4(4Octylphenol);5.4n(4nNonylphenol)3.3,ESI-,,,AESI-,[M-H]-,,,,A,,,AMRM13.4,,A23(LOD),A0.5g/kg2ATable2Linearequations,linearrangesandcorrelationcoefficientsofnonylpheno,loctylphenolandbisphenolAPhenolicxenoestrogensLinearequationsLinearranges(mg/L)CorrelationcoefficientsABisphenolAY=20.66X+8.161~5000.99994tert4tertOctylphenolY=27.53X+118.171~5000.999744NonylphenolY=54.84X+320.851~5000.998844OctylphenolY=69.18X+578.311~5000.99884n4nNonylphenolY=63.02X+339.851~5000.99961992:A3.5A,,,,3(6),86.9%~92.5%,4.9%~9.1%;87.8%~93.0%,4.7%~8.8%33ATable3Resultsofrecoveryfornonylpheno,loctylphenolandbisphenolAintextileandfoodpackagingmaterialsamplesPhenolicxenoestrogensSpikedlevel(g/kg)TextileRecovery(%)RSD(%,n=6)FoodpackagingmaterialRecovery(%)RSD(%,n=6)ABisphenolA0.586.98.288.97.1590.77.790.05.71088.76.591.55.54tert4tertOctylphenol0.589.17.889.18.6587.08.188.56.31089.34.991.04.744Nonylphenol0.588.57.487.86.4592.55.890.67.21091.25.789.35.044Octylphenol0.587.69.191.36.9589.27.591.57.41090.75.488.76.24n4nNonylphenol0.589.29.089.58.8589.98.690.48.11090.36.193.05.83.6T/C4830,6A,5.18~67.5g/kg;134tert,5.24~43.21g/kg;404,47.8~2031g/kg;44n,21A,5.62~190.8g/kg;44tert,5.86~41.1g/kg;244,26.33~3374.32g/kg;44nReferences1WUYongNing(),JIANGGuiBin().TraceandUltratraceInspectionTechnologyofImportantOrganicPollutants(重要有机污染物痕量与超痕量检测技术).Beijing():ChemicalIndustryPress(),2007:5972XIANYanPing(),GUOXinDong(),DUZhiFeng(),LUOHaiYing(),WUYuLuan().ModernFoodScienceandTechnology(现代食品科技),2008,24(5):493~4953CommissionStaffWorkingDocumentonImplementationoftheCommunityStrategyforEndocrineDisruptersARangeofSubstancesSuspectedofInterferingwiththeHormoneSystemsofHumansandWildlife(COM(1999)706)4DUQiaoYun(),GEHong().BaseandApplicationofSurfactants(表面活性剂基础及应用).Beijing():ChinesePetrochemicalPress(),1996:28~315GigerW,BrunnerPH,SchaffnerC.Science,1984,225(4662):623~6256Directive2000/60/ECoftheEuropeanParliamentandoftheCouncilof23October2000EstablishingaFrameworkforCommunityActionintheFieldofWaterPolicy200387OSPARListofChemicalsforPriorityAction(Updated2007).OSPARConventionfortheProtectionoftheMarineEnvironmentoftheNorthEastAtlantic.(Nonylphenol,NonylphenolEthoxylateandCement)9koTexStandard1000,koTexInternationa,lAusgabe/Edition01/200910XIAOJing(),SHAOBing(),WUYongNing(),WANGZhuTian(),YANGJie().ChineseJournalofFoodHygiene(中国食品卫生杂志),2008,20(2):111~11411CHENSuQing(),LIANGHuaDing(),HUANGWeiYa(),HANDeMan(),WANGXiMei().ChineseJ.Anal.Chem.(分析化学),2008,36(7):959~96312WangZD,FingasM.J.Chromatogr.Sci.,1993,31(12):509~51813CAIYaQi(),JIANGGuiBin(),ZHOUQingXiang().Ch